Benzylamine → 2-Benzylamino-6-(t-butylamino)-3-chloro-5-fluoropyridine

HRID 610222노트

반응식

HRID 610222 반응식
[C:1]([NH:5][C:6]1[C:11]([F:12])=[CH:10][C:9]([Cl:13])=[C:8](F)[N:7]=1)([CH3:4])([CH3:3])[CH3:2].[CH2:15]([NH2:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>CN1CCCC1=O>[CH2:15]([NH:22][C:8]1[C:9]([Cl:13])=[CH:10][C:11]([F:12])=[C:6]([NH:5][C:1]([CH3:4])([CH3:3])[CH3:2])[N:7]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

4

반응물 2

HCID 7504BenzylamineHCID 221211892-(t-Butylamino)-5-chloro-3,6-difluoropyridine

생성물 1

HCID 221211832-Benzylamino-6-(t-butylamino)-3-chloro-5-fluoropyridine수율 73.8%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
150 °C

실험 절차

To 10 ml of N-methylpyrrolidone was added 6.8 g of 2-(t-butylamino)-5-chloro-3,6-difluoropyridine together with 8.0 g of benzylamine, and the mixture was stirred at 150° C. for one day, and allowed to cool. After 80 ml of chloroform, the mixture was washed three times with 300 ml of distilled water. The chloroform layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to column chromatography (silica gel, 100 g; eluent: chloroform:n-hexane, 1:1) to obtain about 7.0 g of the title compound as a pale brown crude oil.

후처리

  1. temperatureto cool
  2. washAfter 80 ml of chloroform, the mixture was washed three times with 300 ml of distilled water
  3. dry with materialThe chloroform layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-84977903f248406896fe573dcc873279
출처 데이터셋
uspto-grants-1999_12
특허 번호
US05998436

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